반응 #1435723

ord-8e88224176db4acfa0df229b50d9cf2d

반응 방정식

[Cl-].[Cl-].[Cl-].[Zr+3][CH]1C=CC=C1
cyclopentadienyl zirconium trichloride
Cc1ccccc1
toluene
C[Si](C)(C)OCCC[c-]1cccc1.[K+]
potassium (3-trimethylsiloxypropyl)-cyclopentadienide
Cc1ccccc1
toluene
C[Si](C)(C)OCCC[C]1([Zr+2])C=CC=C1C1C=CC=C1.[Cl-].[Cl-]
[cyclopentadienyl (3-trimethylsiloxypropyl)-cyclopentadienyl]zirconium dichloride

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONis added
  2. 2
    기타A yellow-brown-coloured suspension immediately precipitates
  3. 3
    온도The reaction is maintained for 12 hours
  4. 4
    여과Subsequently, the solution is filtered
  5. 5
    농축concentrated
  6. 6
    기타a crystalline white solid is formed (0.8 g, 2 mmol, 28%)

실험 절차

To a suspension of 2.46 g (7 mmol) of cyclopentadienyl zirconium trichloride in toluene, a suspension of 1.6 g (7 mmol) of potassium (3-trimethylsiloxypropyl)-cyclopentadienide in toluene is added. A yellow-brown-coloured suspension immediately precipitates. The reaction is maintained for 12 hours. Subsequently, the solution is filtered and concentrated and a crystalline white solid is formed (0.8 g, 2 mmol, 28%). 1H-NMR (C6D6): 5.87 (t, 2H), 5.65 (t, 2H), 3.46 (m, 2H), 2.74 (m, 2H), 1.73 (m, 2H), 0.14 (s, 9H). 13C-NMR (C6D6): 11.6.9, 115.0, 114.7, 112.2, 61.8, 33.6, 26.8, −0.393. Mass spectrum: M+-65(356): 30%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07211538B2uspto-grants-2007_05